Potassium Hydroxide → HCID 21323436, compound

HRID 26499Notes

Reaction equation

HRID 26499 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][C:10]3=[N:12][N:13]=[C:14](S(C)(=O)=O)[N:9]3[CH:8]=[CH:7][C:6]=2[CH:19]=1.[OH-:20].[K+]>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][C:10]3=[N:12][NH:13][C:14](=[O:20])[N:9]3[CH:8]=[CH:7][C:6]=2[CH:19]=1

Participants

4

Reactant 2

HCID 14797Potassium HydroxideHCID 21323443HCID 21323443, compound

Product 1

HCID 21323436HCID 21323436, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Conditions

Temperature
95 °C

Procedure

To 2.3 g of 8-chloro-3-methylsulfonyl-11H-s-triazolo[3,4-b][3]benzazepine in 20 ml of dioxane was added 10 ml of 2N-potassium hydroxide and the mixture was heated on a water bath at 95° C. for 30 minutes. The solvent was evaporated off and water was added to the residue. The mixture was made acidic with 2N-HCl and the resultant crystalline precipitate was recovered by filtration and dried. By the above procedure was obtained 8-chloro-2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one as crystals. Recrystallization from chloroform-methanol yielded colorless platelets, m.p. 281°-283° C.

Workup

  1. customThe solvent was evaporated off
  2. additionwater was added to the residue
  3. filtrationthe resultant crystalline precipitate was recovered by filtration
  4. customdried

Sources & evidence

ORD record
ord-df435d2cc2714922874501e40b523364
Source dataset
uspto-grants-1979_04
Patent number
US04150139

Reaction notes

Loading…